高效液相色谱法测定不同产地羌活中紫花前胡苷的含量

目的 :测定不同产地羌活中紫花前胡苷含量。方法 :高效液相色谱法。结果 :紫花前胡苷回归方程为Y=-9509.1+1912709.8X ,r =0.9998,线性范围 0.16～0.64μg ,平均回收率 99.3% ,RSD 2.64%。 结论 :方法简单、快速、重现性好。     

HPLC法测定白花前胡中白花前胡丙素和紫花前胡中紫花前胡苷的含量

目的 :建立高效液相色谱法测定白花前胡根中白花前胡丙素 (dl-praeruptorinA ,Pd -Ia)和紫花前胡根中紫花前胡苷 (nodakenin ,NDK)含量的方法。方法 :色谱柱Shim -PackCLC -ODS ,Pd -Ia的流动相为甲醇 -水 (79∶2 1)和NDK的流动相为乙腈 -甲醇 -水 (2 0∶5∶75 ) ,流速为 1 0mL·min- 1 ,紫外检测波长分别为 32 3和 334nm。结果 :Pd -Ia及NDK的线性范围分别为 0 0 8～ 0 8μg和 0 0 1～ 0 10 μg ,相关系数均为 0 9999,平均回收率分别为 98 5 3%～ 99 2 7%和 97 6 0 %～99 87% ,RSD小于 2 %。结论 :方法准确 ,简便 ,快速 ,灵敏度高 ,对常用中药前胡的质量控制有较重要意义。     

RP-HPLC法同时测定九味羌活丸、片、颗粒中4种成分

目的建立RP-HPLC法同时测定九味羌活丸、片、颗粒(羌活、防风、苍术等)中羌活醇、阿魏酸、异欧前胡素、紫花前胡苷的含有量。方法 3种药物甲醇提取液的分析采用TechMate C18色谱柱(4.6 mm×250 mm,5μm);流动相乙腈-0.1%冰醋酸,梯度洗脱;体积流量1.0 mL/min;柱温35℃;检测波长317 nm。结果羌活醇、阿魏酸、异欧前胡素、紫花前胡苷分别在2.944 2~31.768 2μg/mL(r=0.999 8)、1.995 8~19.958 4μg/mL(r=0.999 8)、2.944 2~29.441 8μg/mL(r=0.999 7)、8.215 0~82.150 1μg/mL(r=0.999 7)范围内线性关系良好,平均加样回收率分别为94.9%、93.9%、91.2%、101.1%,RSD分别为0.9%、1.2%、1.4%、1.0%。结论该方法准确可靠,可用于九味羌活丸、片、颗粒的质量控制。     

经典名方三化汤基准样品量值传递研究

目的 阐明三化汤基准样品的关键质量属性,建立其特征图谱并测定紫花前胡苷、柚皮苷、新橙皮苷、5种游离蒽醌、和厚朴酚与厚朴酚等指标成分,探究三化汤饮片-基准样品量值传递规律,为评价三化汤制剂奠定物质基础。方法 通过文献考证,制备15批三化汤基准样品,采用UPLC建立特征图谱,计算其相似度并确定共有峰归属,结合指标成分及干膏转移率对基准样品进行量值传递分析。结果 建立的15批三化汤基准样品相似度均大于0.98,特征图谱相似度良好,共指认26个共有峰,其中5个来自厚朴,6个来自枳实,5个来自羌活,10个来自大黄;指标成分紫花前胡苷、柚皮苷、新橙皮苷、厚朴酚与和厚朴酚、游离总蒽醌从饮片到基准样品平均转移率分别为（28.08±5.28）%、（45.07±5.35）%、（41.03±4.91）%、（3.32±0.92）%、（16.54±3.57）%,全处方干膏转移率为64.43%～76.39%。结论 采用特征图谱结合多指标成分含量测定及出膏率等评价指标对经典名方三化汤基准样品进行了量值传递综合考察,为三化汤的质量控制和制剂开发提供了科学依据。     

紫花前胡苷在大鼠体内的药代动力学研究

目的研究中药狭叶羌活和宽叶羌活主要化学成分之一的紫花前胡苷(ND)在大鼠体内的药代动力学。方法♂SD大鼠(200～220)g随机分组,每组5只,单次尾静脉注射,给药量为80mg.kg-1,从眼眶静脉丛分时取血、处理。采用反相高效液相色谱法、恒速洗脱,应用外标法测定ND在SD系大鼠血浆中的浓度,应用3P87软件计算主要药代动力学参数。结果在所建立的方法学下,ND的保留时间为6.7min;标准曲线为Y=2.0×10-4X+0.4(r=0.9999),在0.2～80mg.L-1的血浆浓度范围内呈良好的线性关系;血浆中最低检测浓度为0.01mg.L-1(S/N=3),最低定量浓度为0.1mg.L-1(S/N=10);在1.0、10.0和40.0mg.L-1低、中、高3个浓度下的提取回收率为76.23～83.72;日内和日间RSD均小于5.60%(n=3)。在室温和冷冻—解冻试验中,ND具有良好的稳定性。按80mg.kg-1单剂量单次静脉给药后,ND在大鼠体内的药代动力学过程符合开放二房室模型,主要药代动力学参数t1/2α、t1/2β、AUC、Vc、Vp、Vss和CL分别为7.02min、219.27min、1384.34mg.min.L-1、0.92L.kg-1、6.04L.kg-1、6.96L.kg-1和0.06L.kg-1.min-1。结论所建立的方法快速、准确、简便,能够满足ND药代动力学研究要求。按80mg.kg-1单剂量单次静脉给药后,ND在大鼠体内分布广泛,消除速度中等。     

The effects of nodakenin on airway inflammation,hyper-responsiveness and remodeling in a murine model of allergic asthma

Context: Nodakenin is a major coumarin glucoside in the root of Peucedanum decursivum Maxim, a commonly used traditional Chinese medicine for the treatment of asthma and chronic bronchitis for thousands of years.

Objective: In this work, the anti-asthma potential of nodakenin was studied by investigation of its effect to suppress airway inflammation, hyper-responsiveness and remodeling in a murine model of chronic asthma.

Materials and methods: BALB/c mice sensitized to ovalbumin (OVA) were challenged with aerosolized OVA for 8 weeks, orally administered with nodakenin at doses of 5, 10 and 20?mg/kg before each OVA challenge.

Results: Compared with the model group, nodakenin treatment markedly inhibited airway inflammation, hyper-responsiveness and remodeling, showing improvement in subepithelial fibrosis, smooth muscle hypertrophy, and goblet cell hyperplasia, and decreased levels of interleukin (IL)-4, IL-5, IL-13 and matrix metalloproteinase-2/-9 in bronchoalveolar lavage fluid, and the level of OVA-specific IgE in serum. In addition, the NF-κB DNA-binding activity in lung tissues was also reduced by nodakenin treatment.

Conclusions: These data indicated that nodakenin might mitigate the development of chronic experimental allergic asthma.     

薄层扫描法测定羌活中紫花前胡甙的含量

采用双波长薄层扫描法对3种不同产地的羌活中的紫花前胡甙进行含量测定,相关系数为0.9997,加样回收率为97.5%,RSD为1.96%。     

Biotransformation of nodakenin and simultaneous quantification of nodakenin and its aglycone in incubated system of human intestinal bacteria by HPLC method

When nodakenin (1) was anaerobically incubated with human intestinal bacteria, nodakenetin (2) was found as a main biotransformed product. We developed a simple and selective reversed-phase high-performance liquid chromatographic method for simultaneous quantification of 1 and 2 in incubated system of human intestinal bacteria with 1. Chromatographic separation of 1 and 2 was performed on an analytical C₁₈ column, with a mobile phase of MeOH–H₂O (4:6, v/v) at a flow rate of 1.0 ml/min and the UV detection was at 330 nm. The calibration curves were linear over the range of 0.15–24.0 μg/ml for 1 and 0.7–13.2 μg/ml for 2. The lower limits of detection and quantification were 0.01 and 0.1 μg/ml for 1, and 0.005 and 0.05 μg/ml for 2. The recoveries were (87.66 ± 1.66), (79.89 ± 2.53), and (82.96 ± 5.61)% at 1.0, 2.0, and 8.0 μg/ml, respectively, for 1 and (88.32 ± 4.12), (78.15 ± 4.39), and (76.22 ± 3.29)% at 1.0, 4.0, and 16.0 μg/ml, respectively, for 2. The intra- and interday precision and accuracy were validated by relative standard deviation, which were in the ranges of 1.25–4.16 and 2.16–6.12% for 1, and 1.98–6.45 and 2.56–4.57% for 2, respectively. This method has been applied to the simultaneous quantitation of 1 and 2 in incubated system of human intestinal bacteria with 1.     

羌活中二氢呋喃类香豆素在人源肠 Caco-2 细胞单层模型的吸收转运研究

目的 研究紫花前胡苷元 (NANI)、紫花前胡苷 (ND)、前胡苷 V (DEV) 和羌活苷 (FDE) 4个线型二氢呋喃香豆素类化合物在人源肠 Caco-2 细胞单层模型中的吸收特性。方法 利用人源结肠腺癌细胞系 Caco-2 细胞单层模型测试4个香豆素类化合物从绒毛面 (AP 端) 到基底面 (BL 端)、BL 端 到 AP 端2个方向的转运过程。应用偶联紫外检测器的高效液相色谱法对上述4个香豆素进行定量分析,计算转运参数和表观渗透系数(P_app),并与阳性对照药普萘洛尔和阿替洛尔进行比较。结果 NANI 双向转运的 P_app 值在 1×10^-6 cm/s 数量级,介于在 Caco-2 细胞单层模型上呈良好吸收的普萘洛尔和难吸收的阿替洛尔的 P_app 值之间。ND、DEV 和 FDE 的P_app 值与阿替洛尔的P_app 值皆在 1×10^- cm/s 数量级。4个香豆素在 25～400 μmol/L 的转运效率与浓度呈正相关。结论 4个线型二氢呋喃类香豆素可以通过小肠上皮细胞被动吸收进入体内,NANI 属于中等吸收的化合物;ND、DEV 和 FDE 属于难吸收的化合物。     

Coumarin glycosides from the roots ofAngelica dahurica

From the roots ofAngelica dahurica Bentham et Hooker (Umbelliferae), five known coumarin glucosides together with adenosine have been isolated and identified as nodakenin, 3′-hydroxymarmesinin, tert.-O-β-D-glucopyranosyl-byakangelicin, sec.-O-β-D-glucopyranosyl-byakangelicin and scopolin. This is the first report of the occurrence of these compounds in this plant.